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Low yield - A. confusa Options
 
Shunyata
#1 Posted : 12/29/2017 5:00:19 AM
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I thought maybe I wouldn't follow the procedure exactly as indicated. Material from the same source had been used previously with about twice the yield, though maybe there was a variation in alkaloid content.



Approx. l lb. A. confusa root bark powder.



MOD EDIT: removed sourcing talk.



Extraction

The entire batch was put in a large glass container to which about 3 gallons of tap water and vinegar was added.


No heat was applied but allowed to soak for a few days.

The mixture is separated by allowing the fine material to settle to the bottom and decanted off.

More vinegar and water added.

A fish tank heater is used to warm the mixture which is separated after a day or so of soaking.



A lot of sea salt is added until it no longer dissolves in the solution.

This is then separated by emptying out all the liquid except the accumulated salt at the bottom.

After a little bit of time, some precipitate falls to the bottom which is thought to be salt but perhaps this could have contained some alkaloids? Small amount of water is added but the salt is removed.



Basification

A strong solution of KOH and tap water is made.

It’s is slowly added until the entire solution turns black.

A little more is added for good measure.



Extraction:

The solution is heated until it’s barely too hot to handle.

About 250 ml naptha is added, mixed and separated.



The solvent being used has been recycled multiple times from previous extractions.

After the two layers are separated, the naptha is immediately added to a solution of vinegar and water separated and set aside.



The next day there are some alkaloids in the bottle that was used to re-acidify. It is already solid.


This process is repeated 3 times with the same reused naptha.


Basification:

There is about 650 ml of vinegar/water/alkaloid solution.

KOH is added until it turns and remains cloudy/white.

Naptha is used to extract the alkaloids and set aside.



The solution is no longer cloudy.

More KOH is added and turns white again so it is extracted again and a third time but there is not noticeable difference in from the previous extraction.

This second and third extractions are kept separate.



Crystallization:

Naptha #1 is left at room temperature. It’s not long before clear crystals begin to form. They are allowed to continue to grow for 2 days and then moved to the freezer.



Naptha #2:

This one is immediately moved to the freezer for 3 days.



Results:

Both solutions yielded about the same amount of alkaloids. A bit over 1100mg.

Total: 2430mg


The two solutions were combined and put back in the freezer but only resulted in a small qty.
This amount seems rather low for ACRB but maybe it can vary that much?
Perhaps it's human error?

Here are the goods. The one with film looking stuff was the one that went in the freezer immediately.

Shunyata attached the following image(s):
dmtfilm.jpg (112kb) downloaded 91 time(s).
dmtsmallcrystals.jpg (111kb) downloaded 90 time(s).
 

STS is a community for people interested in growing, preserving and researching botanical species, particularly those with remarkable therapeutic and/or psychoactive properties.
 
dmusicaltrancistor
#2 Posted : 12/29/2017 7:01:05 AM

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sourcing talk tsk tskThumbs down

check the attitude section

Attitude
Cubensis Mushroom Colonization Temps 75-80 F Cubensis Mushroom Fruiting Temps 68-74 F
https://ocw.mit.edu/reso...ques-manual-spring-2007/
https://www.dmt-nexus.me...aspx?g=posts&t=36239
cyb wrote:
Xtals are just goo with fancy designer clothes on...
Big grin

 
Shunyata
#3 Posted : 12/29/2017 1:10:03 PM
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Sorry bout the sourcing Crying or very sad ...attitude updated.

Wanted to post a couple pics of the reused solvent though I don't think this would be the problem.

Shunyata attached the following image(s):
clear nap.jpg (81kb) downloaded 69 time(s).
cloudy nap.jpg (69kb) downloaded 69 time(s).
 
dmusicaltrancistor
#4 Posted : 12/29/2017 6:51:31 PM

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thats all good Very happy

what are the 2 layers in that bottle? as in what is the solvent and what is the aqueous liquid?

and plastic isnt really good for holding solvents either
Cubensis Mushroom Colonization Temps 75-80 F Cubensis Mushroom Fruiting Temps 68-74 F
https://ocw.mit.edu/reso...ques-manual-spring-2007/
https://www.dmt-nexus.me...aspx?g=posts&t=36239
cyb wrote:
Xtals are just goo with fancy designer clothes on...
Big grin

 
Shunyata
#5 Posted : 12/29/2017 7:39:13 PM
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The top layer is naptha. It's yellow from repeated use.

The bottom layer is tap water.

Don't have a sep funnel so this is the easiest way I have to separate the layers.
The solution is in the bottle for no more than 30 min.

At first I thought maybe reusing the Sam naptha would be a bad idea but the last pull didn't seem to pull anything so it doesn't seem to matter that much.

The second, cloudy pic is with alkaloids. The second is after shaking the bottle.
 
dmusicaltrancistor
#6 Posted : 12/29/2017 7:48:32 PM

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reusing your naptha is a great idea i generally will always do this

if you dont have a sep funnel that is fine but the plastic will still degrade from the naptha leaching nasty chems into your xtract
you can use a stainless steel or glass turkey baster and keep the solution in a glass or pyrex jar instead of weak plastics also you can use a eyedropper as well just takes more time many of the ecig/vape nicotine juice bottle will have these if you dont have one already maybe ask a friend if he has any empty vape juice bottles

IIRC i think that higher quality plastics are safe for plastic ie. hdpe but that bottle is not good plastic even 30 mins is going to degrade the bottle
Cubensis Mushroom Colonization Temps 75-80 F Cubensis Mushroom Fruiting Temps 68-74 F
https://ocw.mit.edu/reso...ques-manual-spring-2007/
https://www.dmt-nexus.me...aspx?g=posts&t=36239
cyb wrote:
Xtals are just goo with fancy designer clothes on...
Big grin

 
sendokon
#7 Posted : 12/30/2017 2:32:16 AM

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I had troubles for a little while finding the right glass containers. I do cybs so nothing close to the quantity that you mentioned. I use a half gallon glass milk jug from a well know ice cream/milk company. For clean up i use a 800ml Voss "Artiasan" water, found that at a vitamen shop. Figured I'd toss that out there since i saw the plastic bottle.
sendokon attached the following image(s):
20171229_201147.jpg (3,083kb) downloaded 35 time(s).
I can ussually turn a bad trip into somthing positive and take somthing from it and learn. Why is that so diffrent from waking life for me?
 
 
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